阅读说明：本技术 一种气相色谱用液相采进样装置 (Liquid phase sampling device for gas chromatography ) 是由 郭炯远 陆婷婷 华磊 于 2020-12-15 设计创作，主要内容包括：本发明公开了一种气相色谱用液相采进样装置,包括液体定量进样装置和液体气化装置,液体定量进样装置包括由上至下依次设置的阀头以及和阀头连接的阀体,阀体内部设置有贯通阀体顶端和底端的贯通腔,贯通腔内由上至下依次设置有阀瓣以及和阀瓣可拆卸连接的阀杆,液体气化装置包括保温外壳和设置在保温外壳内的加热腔,加热腔内设置有贯穿保温外壳顶端和底端的气化管组,气化管组由内至外嵌套设置有第一气化管、第二气化管和气化管壳体。通过液体定量进样装置向液体气化装置定量输送液体,当样品进入液体气化装置时,可瞬间气化并将气化后的气体输送到色谱柱进行分离,使气相色谱仪能够对液体样品进行分析。(The invention discloses a liquid phase sampling and sampling device for gas chromatography, which comprises a liquid quantitative sampling device and a liquid gasification device, wherein the liquid quantitative sampling device comprises a valve head and a valve body connected with the valve head which are sequentially arranged from top to bottom, a through cavity penetrating through the top end and the bottom end of the valve body is arranged in the valve body, a valve clack and a valve rod detachably connected with the valve clack are sequentially arranged in the through cavity from top to bottom, the liquid gasification device comprises a heat insulation shell and a heating cavity arranged in the heat insulation shell, a gasification pipe group penetrating through the top end and the bottom end of the heat insulation shell is arranged in the heating cavity, and a first gasification pipe, a second gasification pipe and a gasification pipe shell are nested in the gasification. The liquid is quantitatively conveyed to the liquid gasification device through the liquid quantitative sampling device, when a sample enters the liquid gasification device, the sample can be instantly gasified and conveyed to the chromatographic column for separation, so that the gas chromatograph can analyze the liquid sample.)

1. The utility model provides a sampling device is adopted to liquid phase for gas chromatography which characterized in that: the quantitative liquid sampling device (21) is used for quantitatively conveying liquid to the liquid gasification device (22), and the liquid gasification device (22) is used for gasifying the quantitative liquid and conveying the gasified gas to a chromatographic column for analysis;

liquid ration sampling device (21) including valve head (2103) and valve head (2103) swing joint's that from top to bottom set gradually valve body, the inside chamber that link up valve body top and bottom that is provided with of valve body, link up the intracavity from top to bottom set gradually valve clack (2102) and can dismantle valve rod (2101) of being connected with valve clack (2102), valve clack (2102) rotationally set up on the top that links up the chamber, the one end of valve rod (2101) stretches into from the valve body bottom and link up the intracavity and be connected with valve clack (2102) transmission, the other end and the external power device transmission of valve rod (2101) are connected, the one end circumference that valve rod (2101) were kept away from in valve clack (2102) has set gradually first intercommunication groove, second intercommunication groove and third intercommunication groove, the circumference of valve head (2103) is followed in the top of valve head (2103) and has set gradually introduction passageway (2107, The quantitative sampling device comprises a second quantitative ring channel (2112), a vent channel (2110), a sampling channel (2111) and a first quantitative ring channel (2109), wherein the first quantitative ring channel (2109) is communicated with the second quantitative ring channel (2112) through a quantitative ring (2124), a sample feeding channel (2107) is communicated with a liquid sample, a carrier gas channel (2108) is communicated with a carrier gas source, and the vent channel (2110) is communicated with the outside air;

the liquid gasification device (22) comprises a heat-insulating shell (2201) and a heating cavity (2205) arranged in the heat-insulating shell (2201), wherein a gasification tube group penetrating through the top end and the bottom end of the heat-insulating shell (2201) is arranged in the heating cavity (2205), a heating device (2209) is arranged on the inner wall of one end of the heating cavity (2205), a first gasification tube (2206), a second gasification tube (2207) and a gasification tube shell (2210) are nested from inside to outside in the gasification tube group, a gap layer (2208) is formed between the first gasification tube (2206) and the second gasification tube (2207), a sample injection interface (2202) communicated with the first gasification tube (2206) is arranged at the bottom end of the first gasification tube (2206), the bottom end of the sample injection interface (2202) is communicated with a sample injection channel (2107) of the liquid quantitative sampling device (21) through a stainless steel tube, and the top end of the first gasification tube (2206) is lower than the top end of the second gasification tube (2207, the bottom end of the gap layer (2208) is sealed, the top end of the second gasification tube (2207) is provided with a sample outlet interface (2203) communicated with the second gasification tube (2207), the sample outlet interface (2203) is communicated with the chromatographic column, and the outer side wall of the second gasification tube (2207) is provided with a shunt interface (2204) communicated with the gap layer (2208).

2. The liquid sampling and sample introduction device for gas chromatography according to claim 1, characterized in that: the periphery wall of valve body can dismantle from top to bottom in proper order and be provided with first connector (2113), second connector (2114) and disk seat (2115), valve head (2103) be located the top of first connector (2113) and with be provided with the first location boss (2116) and the first positioning groove of looks adaptation between first connector (2113), be provided with the second location boss (2117) and the second positioning groove of looks adaptation between first connector (2113) and second connector (2114), be provided with the third location boss (2118) and the third positioning groove of looks adaptation between second connector (2114) and disk seat (2115).

3. The liquid sampling and sample introduction device for gas chromatography according to claim 2, characterized in that: the valve head (2103), the first connecting body (2113), the second connecting body (2114) and the valve seat (2115) are all provided with through holes which are mutually communicated and coaxial and are fixed through screws.

4. The liquid sampling and sample introduction device for gas chromatography according to claim 2, characterized in that: the valve is characterized in that a butterfly spring (2119), a bearing assembly (2120) and a threaded sleeve (2121) are further arranged in a through cavity of the valve body from top to bottom, the butterfly spring (2119) and the bearing assembly (2120) are sequentially sleeved on the peripheral wall of the valve rod (2101) from top to bottom, the threaded sleeve (2121) is in threaded connection with the valve seat (2115), a positioning flange (2122) is arranged at the top end of the valve rod (2101), the top end of the butterfly spring (2119) is abutted to the bottom end of the positioning flange (2122), and the bottom end of the bearing assembly (2120) is supported at the top end of the threaded sleeve (2121).

5. The liquid sampling and sample introduction device for gas chromatography according to claim 1, characterized in that: a plurality of positioning pins are arranged between the valve clack (2102) and the valve rod (2101), a plurality of upper half pin holes are formed in the bottom end of the valve clack (2102), a plurality of lower half pin holes corresponding to the upper half pin holes in position are formed in the top end of the valve rod (2101), one end of each positioning pin is arranged in each upper half pin hole, and the other end of each positioning pin is arranged in the corresponding lower half pin hole.

6. The liquid sampling and sample introduction device for gas chromatography according to claim 1, characterized in that: the sample inlet interface (2202), the sample outlet interface (2203) and the shunt interface (2204) are all hollow cylindrical structures.

7. The liquid sampling and sample introduction device for gas chromatography according to claim 1, characterized in that: the quantitative loop (2124) is a 1uL quantitative loop.

8. The liquid sampling and sample introduction device for gas chromatography according to claim 1, characterized in that: the heating device (2209) is a heating rod, the power device is a rotary cylinder, and an output shaft of the rotary cylinder is connected with one end, far away from the valve head, of the valve rod (2101).

Technical Field

The invention relates to the field of sampling and sample introduction, in particular to a liquid phase sampling and sample introduction device for gas chromatography.

Background

Gas chromatographs on the existing market are based on gas analysis, use classical gas injection valves, and the gas injection valves can relatively easily ensure that a gas sample of 1ml is basically delivered to a separation detection system of the gas chromatograph every time, and are mainly applied to detection of atmospheric pollution, industrial waste gas emission and the like. For the analysis of primary liquid, finished product and waste liquid in the chemical industry, because of the lack of a liquid gasification sample injection device, 1ul of almost invisible liquid sample is difficult to be automatically sent to a capillary sample injector and then gasified, shunted, injected and detected, and can be analyzed on a laboratory gas chromatograph after being manually sampled, so that how to analyze the liquid sample by the gas chromatograph becomes the problem to be solved by technical personnel in the field at present.

Disclosure of Invention

In order to solve the above problems in the prior art, an object of the present invention is to provide a liquid sampling apparatus for gas chromatography, which enables a gas chromatograph to analyze a liquid sample.

In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a liquid sampling and sampling device for gas chromatography comprises a liquid quantitative sampling device and a liquid gasification device, wherein the liquid quantitative sampling device quantitatively conveys liquid to the liquid gasification device, and the liquid gasification device gasifies the quantitative liquid and conveys the gasified gas to a chromatographic column for analysis;

the liquid quantitative sampling device comprises a valve head and a valve body movably connected with the valve head, wherein a through cavity which penetrates through the top end and the bottom end of the valve body is arranged inside the valve body, a valve clack and a valve rod detachably connected with the valve clack are sequentially arranged in the through cavity from top to bottom, the valve clack is rotatably arranged at the top end of the through cavity, one end of the valve rod extends into the through cavity from the bottom end of the valve body and is connected with the valve clack in a transmission way, the other end of the valve rod is connected with an external power device in a transmission way, a first connecting groove, a second connecting groove and a third connecting groove are sequentially arranged at the circumferential direction of one end, far away from the valve rod, of the valve clack, a sampling channel, a carrier gas channel, a second quantitative ring channel, an emptying channel, a sampling channel and a first quantitative ring channel are sequentially arranged at the top, the sample introduction channel is communicated with the liquid sample, the carrier gas channel is communicated with a carrier gas source, and the emptying channel is communicated with the outside air;

the liquid gasification device comprises a heat-insulating shell and a heating cavity arranged in the heat-insulating shell, wherein a gasification pipe group penetrating through the top end and the bottom end of the heat-insulating shell is arranged in the heating cavity, the inner wall of one end of the heating cavity is provided with a heating device, the gasification pipe group is provided with a first gasification pipe, a second gasification pipe and a gasification pipe shell in an embedded manner from inside to outside, and a gap layer is formed between the first gasification tube and the second gasification tube, the bottom end of the first gasification tube is provided with a sample introduction interface communicated with the first gasification tube, the bottom end of the sample introduction interface is communicated with a sample introduction channel of the liquid quantitative sample introduction device through a stainless steel tube, the top end of the first gasification tube is lower than the top end of the second gasification tube, the bottom end of the gap layer is blocked, the top end of the second gasification tube is provided with a sample outlet interface communicated with the second gasification tube, the sample outlet interface is communicated with the chromatographic column, and the outer side wall of the second gasification tube is provided with a shunt interface communicated with the gap layer.

As a further improvement of the invention, a first connecting body, a second connecting body and a valve seat are detachably arranged on the peripheral wall of the valve body from top to bottom in sequence, the valve head is positioned at the top end of the first connecting body, a first positioning boss and a first positioning groove which are matched with each other are arranged between the valve head and the first connecting body, a second positioning boss and a second positioning groove which are matched with each other are arranged between the first connecting body and the second connecting body, and a third positioning boss and a third positioning groove which are matched with each other are arranged between the second connecting body and the valve seat.

As a further improvement of the invention, the valve head, the first connecting body, the second connecting body and the valve seat are all provided with through holes which are mutually communicated and coaxial and are fixed by screws.

As a further improvement of the invention, a butterfly spring, a bearing assembly and a threaded sleeve are further arranged in the through cavity of the valve body from top to bottom, the butterfly spring and the bearing assembly are sequentially sleeved on the peripheral wall of the valve rod from top to bottom, the threaded sleeve is in threaded connection with the valve seat, a positioning flange is arranged at the top end of the valve rod, the top end of the butterfly spring is abutted against the bottom end of the positioning flange, and the bottom end of the bearing assembly is supported at the top end of the threaded sleeve.

As a further improvement of the invention, a plurality of positioning pins are arranged between the valve clack and the valve rod, a plurality of upper half pin holes are arranged at the bottom end of the valve clack, a plurality of lower half pin holes corresponding to the upper half pin holes are arranged at the top end of the valve rod, one end of each positioning pin is respectively arranged in the upper half pin holes, and the other end of each positioning pin is arranged in the corresponding lower half pin holes.

As a further improvement of the invention, the sample inlet interface, the sample outlet interface and the shunt interface are all hollow cylindrical structures.

As a further improvement of the invention, the quantitative ring is a 1ul ring

As a further improvement of the invention, the heating device is a heating rod, the power device is a rotary cylinder, and an output shaft of the rotary cylinder is connected with one end of the valve rod, which is far away from the valve head.

Compared with the prior art, the invention has the following beneficial effects:

1. the liquid is quantitatively conveyed to the liquid gasification device through the liquid quantitative sampling device, when a sample enters the liquid gasification device, the sample can be instantly gasified and conveyed to the chromatographic column for separation, so that the gas chromatograph can analyze the liquid sample.

2. Through setting up belleville spring, bearing assembly and thread bush, stationarity is better when making the valve rod rotate.

3. Through setting up mutual detachable valve head, first connector, second connector and disk seat, it is more convenient to make the dismouting of liquid ration sampling device.

4. Through setting up 1uL trace ration ring messenger sample volume repeatability is good, and liquid sample is not impermeable, has guaranteed the repeatability of advancing the appearance at every turn, and the ration is accurate.

Drawings

FIG. 1 is a sectional view of a quantitative liquid sample injection device according to the present invention;

FIG. 2 is a top view of the quantitative liquid sample injection device of the present invention;

FIG. 3 is a sectional view of a liquid vaporizer according to the present invention;

FIG. 4 is a schematic view of the combination of the quantitative liquid feeding device and the liquid vaporizing device;

in the drawings: 21. a liquid quantitative sample introduction device; 2101. a valve stem; 2102. a valve flap; 2103. a valve head; 2107. a sample introduction channel; 2108. a carrier gas channel; 2109. a first dosing ring channel; 2110. emptying the channel; 2111. a sampling channel; 2112. a second dosing ring channel; 2113. a first connecting body; 2114. a second connector; 2115. a valve seat; 2116. a first positioning boss; 2117. a second positioning boss; 2118. a third positioning boss; 2119. a belleville spring; 2120. a bearing assembly; 2121. a threaded sleeve; 2122. a positioning flange; 2124. a dosing ring;

22. a liquid vaporizing device; 2201. a heat-insulating shell; 2202. a sample introduction interface; 2203. a sample outlet interface; 2204. a shunt interface; 2205. a heating cavity; 2206. a first gasification pipe; 2207. a second vaporizing tube; 2208. a gap layer; 2209. a heating device; 2210. a gasification tube housing.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The invention relates to a liquid phase sampling and sampling device for gas chromatography, which comprises a liquid quantitative sampling device 21 and a liquid gasification device 22, wherein the liquid quantitative sampling device 21 quantitatively conveys liquid to the liquid gasification device 22, and the liquid gasification device 22 gasifies the quantitative liquid and conveys the gasified gas to a chromatographic column for analysis;

the liquid quantitative sampling device 21 comprises a valve head 2103 and a valve body movably connected with the valve head 2103, wherein the valve body is internally provided with a through cavity which penetrates through the top end and the bottom end of the valve body, a valve flap 2102 and a valve rod 2101 detachably connected with the valve flap 2102 are sequentially arranged in the through cavity from top to bottom, the valve flap 2102 is rotatably arranged at the top end of the through cavity, one end of the valve rod 2101 extends into the through cavity from the bottom end of the valve body and is in transmission connection with the valve flap 2102, the other end of the valve rod 2101 is in transmission connection with an external power device, a first connecting groove, a second connecting groove and a third connecting groove are sequentially arranged at one end, far away from the valve rod 2101, of the valve flap 2102 in the circumferential direction, the top end of the valve head 2103 is sequentially provided with a sampling channel 2107, a carrier gas channel 2108, a second quantitative ring channel 2102, an emptying channel 2110, a, the first quantitative ring channel 2109 is communicated with the second quantitative ring channel 2112 through a quantitative ring 2124, the sample injection channel 2107 is communicated with a liquid sample, the carrier gas channel 2108 is communicated with a carrier gas source, and the emptying channel 2110 is communicated with the outside air;

the liquid gasification device 22 comprises a heat-insulating casing 2201 and a heating cavity 2205 arranged in the heat-insulating casing 2201, wherein a gasification tube group penetrating through the top end and the bottom end of the heat-insulating casing 2201 is arranged in the heating cavity 2205, a heating device 2209 is arranged on the inner wall of one end of the heating cavity 2205, a first gasification tube 2206, a second gasification tube 2207 and a gasification tube shell 2210 are nested from inside to outside in the gasification tube group, a gap layer 2208 is formed between the first gasification tube 2206 and the second gasification tube 2207, a sample inlet 2202 communicated with the first gasification tube 2206 is arranged at the bottom end of the first gasification tube 2206, the bottom end of the sample inlet 2202 is communicated with a sample inlet passage 2107 of the liquid quantitative sample injection device 21 through a stainless steel tube, the top end of the first gasification tube 2206 is lower than the top end of the second gasification tube 2207, the bottom end of the gap layer 2208 is sealed, a sample outlet 2203 communicated with the second gasification tube 2207 is arranged at the top end, the sample outlet port 2203 is communicated with the chromatographic column, and a flow splitting port 2204 communicated with the gap layer 2208 is arranged on the outer side wall of the second gasification pipe 2207.

Sampling state: as shown in fig. 1, fig. 2, and fig. 4, the sampling channel 2111 is communicated with the first quantitative ring channel 2109 through a first communicating groove, the sample feeding channel 2107 is communicated with the carrier gas channel 2108 through a second communicating groove, and the second quantitative ring channel 2112 is communicated with the emptying channel 2110 through a third communicating groove, and the formed channel is: liquid sample → sampling channel 2111 → first connecting channel → first dosing ring channel 2109 → second dosing ring channel 2112 → third connecting channel → vent channel 2110. The sampling phase ends when the dosing ring 2124 is filled with the liquid sample to be measured.

Sample introduction state: as shown in fig. 1, fig. 2, fig. 3, and fig. 4, after the sampling stage is ended, the power device drives the valve rod 2101 to rotate, the valve rod 2101 drives the valve flap 2102 to rotate synchronously, when the valve flap 2102 rotates to the first quantitative ring channel 2109 and is communicated with the sample injection channel 2107 through the first communicating groove, the carrier gas channel 2108 is communicated with the second quantitative ring channel 2112 through the second communicating groove, and the emptying channel 2110 is communicated with the sampling channel 2111 through the third communicating groove, and is switched to the sample injection state, where the formed path 2110 is: the carrier gas source → the carrier gas channel 2108 → the second communicating groove → the second quantitative ring channel 2112 → the first quantitative ring channel 2109 → the first communicating groove → the sample feeding channel 2107. The liquid sample to be measured filled in the quantitative ring 2124 enters the sample inlet 2202 of the liquid vaporizing device 22 under the driving of the carrier gas, and enters the first vaporizing tube 2206 from the sample inlet 2202, at this time, under the action of the heating device 2209, the heating cavity 2205 is in a high-temperature state, the first vaporizing tube 2206 penetrates through the heating cavity 2205, the part of the first vaporizing tube 2206 located in the heating cavity 2205 is also in the high-temperature state, the liquid sample is vaporized instantaneously in the process of passing through the part, the volume of the sample is expanded after being vaporized, a part of the expanded gas enters the chromatographic column from the sample outlet 2203, and the other part of the expanded gas enters the gap layer 2208 from the top end of the first vaporizing tube 2206 and descends along the gap layer 2208, and after reaching the shunt interface 2204, the gas is discharged from the shunt interface 2204 through the vaporizing tube housing 2210.

As shown in fig. 1, the peripheral wall of the valve body is sequentially detachably provided with a first connector 2113, a second connector 2114 and a valve seat 2115 from top to bottom, the valve head 2103 is located at the top end of the first connector 2113 and is provided with a first positioning boss 2116 and a first positioning groove which are matched with each other between the first connector 2113, a second positioning boss 2117 and a second positioning groove which are matched with each other are provided between the first connector 2113 and the second connector 2114, and a third positioning boss 2118 and a third positioning groove which are matched with each other are provided between the second connector 2114 and the valve seat 2115. Valve head 2103, first connector 2113, second connector 2114 and valve seat 2115 all set up the through-hole that link up each other and coaxial and pass through the screw fixation, and the dismouting is more convenient.

As shown in fig. 1, a belleville spring 2119, a bearing assembly 2120 and a threaded sleeve 2121 are further arranged in the through cavity of the valve body from top to bottom, the belleville spring 2119 and the bearing assembly 2120 are sequentially sleeved on the peripheral wall of the valve rod 2101 from top to bottom, the threaded sleeve 2121 is in threaded connection with the valve seat 2115, a positioning flange 2122 is arranged at the top end of the valve rod 2101, the top end of the belleville spring 2119 abuts against the bottom end of the positioning flange 2122, and the bottom end of the bearing assembly 2120 is supported at the top end of the threaded sleeve 2121. The valve rod 2101 is more rotationally smooth by the arrangement of the belleville spring 2119, the bearing assembly 2120 and the threaded sleeve 2121.

Specifically, a plurality of positioning pins are arranged between the valve clack 2102 and the valve rod 2101, a plurality of upper half pin holes are formed in the bottom end of the valve clack 2102, a plurality of lower half pin holes corresponding to the upper half pin holes are formed in the top end of the valve rod 2101, one end of each positioning pin is arranged in the upper half pin hole, the other end of each positioning pin is arranged in the corresponding lower half pin hole, and the device is more convenient to disassemble and assemble.

Specifically, the sample inlet port 2202, the sample outlet port 2203, and the flow dividing port 2204 are all hollow cylindrical structures.

Specifically, the quantitative ring 2124 is a 1ul quantitative ring. The micro quantitative ring ensures that the sample injection amount has good repeatability and the liquid sample cannot permeate, thereby ensuring the repeatability of each sample injection and having accurate quantification. The liquid quantitative sampling device 21 switches 1ul of liquid sample each time and cuts into the first gasification tube 2206, the liquid sample is gasified instantly after entering the first gasification tube 2206, and enters the chromatographic column along the first gasification tube 2206 to realize separation.

Specifically, the heating device 2209 is a heating rod, the power device is a rotary cylinder, an output shaft of the rotary cylinder is connected with one end, far away from the valve head, of the valve rod 2101, and the valve rod is driven to be integrally switched to a sample injection state when the cylinder is switched.

Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.